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US6525343B1 - Micro-chip for chemical reaction - Google Patents

Micro-chip for chemical reaction Download PDF

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Publication number
US6525343B1
US6525343B1 US09/890,877 US89087701A US6525343B1 US 6525343 B1 US6525343 B1 US 6525343B1 US 89087701 A US89087701 A US 89087701A US 6525343 B1 US6525343 B1 US 6525343B1
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US
United States
Prior art keywords
chemical reaction
chemical
reaction pool
microchip
portions
Prior art date
Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
Expired - Fee Related
Application number
US09/890,877
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English (en)
Inventor
Michifumi Tanga
Current Assignee (The listed assignees may be inaccurate. Google has not performed a legal analysis and makes no representation or warranty as to the accuracy of the list.)
Toyo Kohan Co Ltd
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Toyo Kohan Co Ltd
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Filing date
Publication date
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Assigned to TOYO KOHAN CO., LTD. reassignment TOYO KOHAN CO., LTD. ASSIGNMENT OF ASSIGNORS INTEREST (SEE DOCUMENT FOR DETAILS). Assignors: TANGA, MICHIFUMI
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    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
    • B01J19/00—Chemical, physical or physico-chemical processes in general; Their relevant apparatus
    • B01J19/0093—Microreactors, e.g. miniaturised or microfabricated reactors
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
    • B01J19/00—Chemical, physical or physico-chemical processes in general; Their relevant apparatus
    • B01J19/0046—Sequential or parallel reactions, e.g. for the synthesis of polypeptides or polynucleotides; Apparatus and devices for combinatorial chemistry or for making molecular arrays
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01L—CHEMICAL OR PHYSICAL LABORATORY APPARATUS FOR GENERAL USE
    • B01L3/00—Containers or dishes for laboratory use, e.g. laboratory glassware; Droppers
    • B01L3/50—Containers for the purpose of retaining a material to be analysed, e.g. test tubes
    • B01L3/502—Containers for the purpose of retaining a material to be analysed, e.g. test tubes with fluid transport, e.g. in multi-compartment structures
    • B01L3/5027—Containers for the purpose of retaining a material to be analysed, e.g. test tubes with fluid transport, e.g. in multi-compartment structures by integrated microfluidic structures, i.e. dimensions of channels and chambers are such that surface tension forces are important, e.g. lab-on-a-chip
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
    • B01J2219/00—Chemical, physical or physico-chemical processes in general; Their relevant apparatus
    • B01J2219/00274—Sequential or parallel reactions; Apparatus and devices for combinatorial chemistry or for making arrays; Chemical library technology
    • B01J2219/00277—Apparatus
    • B01J2219/00279—Features relating to reactor vessels
    • B01J2219/00306—Reactor vessels in a multiple arrangement
    • B01J2219/00313—Reactor vessels in a multiple arrangement the reactor vessels being formed by arrays of wells in blocks
    • B01J2219/00315—Microtiter plates
    • B01J2219/00317—Microwell devices, i.e. having large numbers of wells
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
    • B01J2219/00—Chemical, physical or physico-chemical processes in general; Their relevant apparatus
    • B01J2219/00274—Sequential or parallel reactions; Apparatus and devices for combinatorial chemistry or for making arrays; Chemical library technology
    • B01J2219/00277—Apparatus
    • B01J2219/00495—Means for heating or cooling the reaction vessels
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
    • B01J2219/00—Chemical, physical or physico-chemical processes in general; Their relevant apparatus
    • B01J2219/00781—Aspects relating to microreactors
    • B01J2219/00783—Laminate assemblies, i.e. the reactor comprising a stack of plates
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
    • B01J2219/00—Chemical, physical or physico-chemical processes in general; Their relevant apparatus
    • B01J2219/00781—Aspects relating to microreactors
    • B01J2219/00873—Heat exchange
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01L—CHEMICAL OR PHYSICAL LABORATORY APPARATUS FOR GENERAL USE
    • B01L2300/00—Additional constructional details
    • B01L2300/08—Geometry, shape and general structure
    • B01L2300/0861—Configuration of multiple channels and/or chambers in a single devices
    • B01L2300/087—Multiple sequential chambers
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01L—CHEMICAL OR PHYSICAL LABORATORY APPARATUS FOR GENERAL USE
    • B01L2300/00—Additional constructional details
    • B01L2300/12—Specific details about materials
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01L—CHEMICAL OR PHYSICAL LABORATORY APPARATUS FOR GENERAL USE
    • B01L2300/00—Additional constructional details
    • B01L2300/18—Means for temperature control
    • B01L2300/1805—Conductive heating, heat from thermostatted solids is conducted to receptacles, e.g. heating plates, blocks
    • B01L2300/1822—Conductive heating, heat from thermostatted solids is conducted to receptacles, e.g. heating plates, blocks using Peltier elements
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01L—CHEMICAL OR PHYSICAL LABORATORY APPARATUS FOR GENERAL USE
    • B01L2400/00—Moving or stopping fluids
    • B01L2400/04—Moving fluids with specific forces or mechanical means
    • B01L2400/0403—Moving fluids with specific forces or mechanical means specific forces
    • B01L2400/0406—Moving fluids with specific forces or mechanical means specific forces capillary forces
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01L—CHEMICAL OR PHYSICAL LABORATORY APPARATUS FOR GENERAL USE
    • B01L2400/00—Moving or stopping fluids
    • B01L2400/06—Valves, specific forms thereof
    • B01L2400/0633—Valves, specific forms thereof with moving parts
    • B01L2400/0661—Valves, specific forms thereof with moving parts shape memory polymer valves
    • C—CHEMISTRY; METALLURGY
    • C40—COMBINATORIAL TECHNOLOGY
    • C40B—COMBINATORIAL CHEMISTRY; LIBRARIES, e.g. CHEMICAL LIBRARIES
    • C40B60/00—Apparatus specially adapted for use in combinatorial chemistry or with libraries
    • C40B60/14—Apparatus specially adapted for use in combinatorial chemistry or with libraries for creating libraries
    • G—PHYSICS
    • G01—MEASURING; TESTING
    • G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
    • G01N35/00—Automatic analysis not limited to methods or materials provided for in any single one of groups G01N1/00 - G01N33/00; Handling materials therefor
    • G01N35/00029—Automatic analysis not limited to methods or materials provided for in any single one of groups G01N1/00 - G01N33/00; Handling materials therefor provided with flat sample substrates, e.g. slides
    • G01N2035/00099—Characterised by type of test elements
    • G01N2035/00158—Elements containing microarrays, i.e. "biochip"
    • G—PHYSICS
    • G01—MEASURING; TESTING
    • G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
    • G01N35/00—Automatic analysis not limited to methods or materials provided for in any single one of groups G01N1/00 - G01N33/00; Handling materials therefor
    • G01N35/08—Automatic analysis not limited to methods or materials provided for in any single one of groups G01N1/00 - G01N33/00; Handling materials therefor using a stream of discrete samples flowing along a tube system, e.g. flow injection analysis
    • Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
    • Y10—TECHNICAL SUBJECTS COVERED BY FORMER USPC
    • Y10S—TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
    • Y10S257/00—Active solid-state devices, e.g. transistors, solid-state diodes
    • Y10S257/93—Thermoelectric, e.g. peltier effect cooling

Definitions

  • the present invention relates to a microchip for a chemical reaction in which various types of chemical reactions can be performed in a microspace.
  • Such an integrated chemical laboratory is constituted by forming a process channel of from sub- ⁇ m to 100 ⁇ m on a glass substrate having a size of several centimeters square and has an object of performing a chemical reaction on a micro level, separate and, further, detecting a resultant reaction product in a continuous operation.
  • the glass substrate is low in thermal resistance, there is a fear that an experiment cannot be executed at high temperature.
  • the present invention can solve the above-described problems and has an object of providing a microchip for a chemical reaction in which an experiment can be executed in a quick manner irrespective of a type of a chemical substance to be subjected to a chemical reaction and under all experimental conditions.
  • a microchip for a chemical reaction is constituted such that a plurality of chemical reaction pool portions and a horizontal communication path composed of a channel which communicates and connects the plurality of chemical reaction pool portions with each other are formed on the surface of a diamond substrate of a minute size.
  • a vertical communication path composed of a pass-through hole which vertically communicates with one of the chemical reaction pool portions is provided and an opening/closing valve is attached to a communication and connection portion.
  • a heating/cooling means is attached along a periphery or a bottom surface of the chemical reaction pool portions for the purpose of heating/cooling the chemical reaction portions.
  • FIG. 1 is a perspective view of a microchip for a chemical reaction according to an embodiment of the present invention
  • FIG. 2 is a plan view of a microchip for a chemical reaction according to an embodiment of the present invention
  • FIG. 3 is a sectional view taken on line I—I of FIG. 2;
  • FIG. 4 is a sectional view of a microchip for a chemical reaction according to an embodiment of the present invention in a state in which a heating/cooling means is attached;
  • FIG. 5 is an explanatory view of production processes of a diamond substrate of a microchip for a chemical reaction according to an embodiment of the present invention.
  • a diamond substrate 10 which comprises the main body of the microchip A for the chemical reaction is made of a rectangular plate having a width and length of several cm each and a thickness of sub- ⁇ m to several hundred ⁇ m. And, on the surface of a side of the diamond substrate 10 , are formed a plurality of chemical reaction pool portions 11 , 12 and a horizontal communication path 13 composed of a channel which communicates and connects these chemical reaction pool portions 11 , 12 therebetween.
  • horizontal communication paths 18 , 19 composed of channels for communicating and connecting chemical reaction pool portions 16 , 17 which have similarly been provided in respective diamond substrates 14 , 15 of other microchips A 1 , A 2 for chemical reactions that are placed adjacent to the microchip A for the chemical reaction on a horizontal plane with the chemical reaction pool portions 11 , 12 of the microchip A for the chemical reaction, respectively.
  • a vertical communication path 20 composed of a pass-through hole for vertically communicating and connecting with the chemical reaction pool portion 11 ; attached is an opening/closing valve 21 to a communication and connection portion between the chemical reaction pool portion 11 and the vertical communication path 20 . Therefore, as shown in FIG. 3, the chemical reaction pool portion 11 can be communicated and connected with a chemical reaction pool portion 22 provided on a diamond substrate 22 a of a microchip A 3 for a chemical reaction which is provided under the microchip A for the chemical reaction and, further, communication therebetween can be cut off by closing the opening/closing valve 21 .
  • the opening/closing valve 21 can be formed from, for example, a valve plate having a property of shape-memory alloy.
  • a heating/cooling means 23 , 24 such as a Peltier device can be attached to portions which correspond to the chemical reaction pool portions 11 , 12 under the diamond substrate 10 of the microchip A for the chemical reaction.
  • a heating/cooling means 23 , 24 such as a Peltier device can be attached to portions which correspond to the chemical reaction pool portions 11 , 12 under the diamond substrate 10 of the microchip A for the chemical reaction.
  • a plurality of chemical substances in liquid, gas and solid forms which are subjected to experiments are each flowed or introduced into the chemical reaction pool portion 11 to effect a chemical reaction and after the reaction the resulting product is sent to the chemical reaction pool portion 12 or the chemical reaction pool portion 22 through the horizontal communication path 13 or the vertical communication path 20 where a subsequent chemical reaction, a component analysis or the like is performed.
  • substrates of the microchips A, A 3 (same is also applicable to A 1 , A 2 ) for the chemical reactions are composed of diamond substrates 10 , 22 a ( 14 , 15 ), they have high corrosion resistance to all chemical substances and can perform a variety of chemical experiments in respective microspaces thereof free of restrictions irrespective of types of chemical substances.
  • the diamond substrates 10 , 14 , 15 , 22 a are excellent in thermal conductivity, for example, the heating/cooling means 23 , 24 such as a Peltier device and the like are attached to portions corresponding to the chemical reaction pool portions 11 , 12 to enhance a chemical reaction rate thereby efficiently executing an experiment.
  • the heating/cooling means 23 , 24 such as a Peltier device and the like are attached to portions corresponding to the chemical reaction pool portions 11 , 12 to enhance a chemical reaction rate thereby efficiently executing an experiment.
  • the chemical reaction pool portions 11 , 12 , 16 , 17 , 22 can be formed and machined by melting and removing by means of a diamond laser or the like; however, as is described below with reference to FIGS. 5, the chemical reaction pool portions 11 , 12 , 16 , 17 , 22 having a clear cross-section can be formed on silicon 30 by a transfer method.
  • a silicon oxide film 31 is grown on the surface of the silicon 30 .
  • patterning is performed using a photoresist 30 a .
  • the silicon oxide film 31 is removed by performing isotropic etching using hydrofluoric acid (HF).
  • the silicon 30 is subjected to anisotropic etching using a tetramethylammoniumhydroxide solution ((CH 3 ) 4 NOH).
  • a tetramethylammoniumhydroxide solution ((CH 3 ) 4 NOH).
  • diamond 33 is grown by a hot-filament CVD method. After the diamond 33 is grown, the surface of a thus-grown diamond 33 is coated with electroconductive epoxy 33 a which is then placed on a platinum plate and fixed thereto by being hardened by heat.
  • the silicon substrate 32 is removed in a mixture of hydrofluoric acid and nitric acid (HF+HNO 3 ) to form chemical reaction pool portions 11 , 12 , 16 , 17 and 22 .
  • HF+HNO 3 hydrofluoric acid and nitric acid
  • a method of forming the silicon substrate 32 in a trapezoid state as a mold there is also a method in which, instead of growing the silicon oxide film 31 on the surface of the silicon 30 described with reference to FIG. 5 ( a ), patterning is performed on the silicon substrate using the photoresist. Further, there is a method of etching a silicon surface using sulfur hexafluoride as an etching gas by means of an RIE (reactive ion etching) method, instead of performing the etching using hydrofluoric acid (HF) as described with reference to FIG. 5 ( b ). Thereafter, these methods are followed by a process of growing diamond 33 by the hot-filament CVD method as shown in the above-described FIG. 5 ( d ).
  • RIE reactive ion etching
  • the substrate of the microchip since a diamond substrate is used as a substrate of a microchip for a chemical reaction, the substrate of the microchip has a high resistance to all types of chemical substances and a variety of experiments can be conducted in a microspace thereof without being restricted by types of chemical substances in a manner different from a glass substrate.
  • a vertical communication path for vertically communicating and connecting with a chemical reaction pool portion and an opening/closing valve in a communication and connection portion thereby forming a three-dimensional chemical experiment facility in a compact space of which a variety of experiments can be conducted.
  • the diamond substrate is excellent in thermal conductivity, a provision of a heatig/cooling means such as Peltier device and the on a portion corresponding to the chemical reaction pool portion enhances a reaction rate, thereby efficiently conducting the experiment.
  • a heatig/cooling means such as Peltier device and the on a portion corresponding to the chemical reaction pool portion enhances a reaction rate, thereby efficiently conducting the experiment.

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  • Chemical & Material Sciences (AREA)
  • Organic Chemistry (AREA)
  • Chemical Kinetics & Catalysis (AREA)
  • Health & Medical Sciences (AREA)
  • General Health & Medical Sciences (AREA)
  • Analytical Chemistry (AREA)
  • Dispersion Chemistry (AREA)
  • Hematology (AREA)
  • Clinical Laboratory Science (AREA)
  • Physical Or Chemical Processes And Apparatus (AREA)
  • Micromachines (AREA)
  • Crystals, And After-Treatments Of Crystals (AREA)
  • Automatic Analysis And Handling Materials Therefor (AREA)
  • Devices For Use In Laboratory Experiments (AREA)
US09/890,877 1999-02-18 2000-02-16 Micro-chip for chemical reaction Expired - Fee Related US6525343B1 (en)

Applications Claiming Priority (3)

Application Number Priority Date Filing Date Title
JP11-040689 1999-02-18
JP4068999 1999-02-18
PCT/JP2000/000867 WO2000048724A1 (fr) 1999-02-18 2000-02-16 Microcircuit integre pour reaction chimique

Publications (1)

Publication Number Publication Date
US6525343B1 true US6525343B1 (en) 2003-02-25

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Country Status (7)

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US (1) US6525343B1 (fr)
EP (1) EP1174182A4 (fr)
KR (1) KR100630297B1 (fr)
CN (1) CN1150059C (fr)
AU (1) AU2571600A (fr)
CA (1) CA2371767C (fr)
WO (1) WO2000048724A1 (fr)

Cited By (8)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
US20040028562A1 (en) * 2000-11-29 2004-02-12 Thomas Greve Device for controlling the temperature of microcomponents
US20050006372A1 (en) * 2003-07-10 2005-01-13 Citizen Watch Co., Ltd Temperature regulator for microchemical chip
US20070116614A1 (en) * 2005-09-20 2007-05-24 Yamaha Corporation Temperature control apparatus for microchemical chip
US20080047836A1 (en) * 2002-12-05 2008-02-28 David Strand Configurable Microfluidic Substrate Assembly
US20130015254A1 (en) * 2011-07-13 2013-01-17 GM Global Technology Operations LLC Temperature dependent variable flow orifice
US20140227147A1 (en) * 2013-02-08 2014-08-14 Infineon Technologies Ag Microfluidic Device and Method
USD844805S1 (en) 2016-02-29 2019-04-02 President And Fellows Of Harvard College Holder
USD846755S1 (en) * 2016-12-07 2019-04-23 President And Fellows Of Harvard College Holder

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JP4954386B2 (ja) * 2001-05-07 2012-06-13 財団法人神奈川科学技術アカデミー 電場または磁場印加によるマイクロチップ液液界面反応方法とそのためのマイクロチップ
US7419822B2 (en) * 2002-10-04 2008-09-02 Noo Li Jeon Microfluidic device for enabling fluidic isolation among interconnected compartments within the apparatus and methods relating to same
EP1510253A1 (fr) * 2003-08-21 2005-03-02 Yamaha Corporation Microreacteur et procédé de production de substance avec un tel microreacteur
JP2005114298A (ja) * 2003-10-10 2005-04-28 Citizen Watch Co Ltd 温度調節装置
EP1711264B1 (fr) * 2004-02-02 2010-03-31 Silicon Valley Scientific, Inc. Systeme integre equipe de composants microfluidiques modulaires
US8444934B2 (en) * 2004-03-26 2013-05-21 Universite Laval Removable microfluidic flow cell
DE102004050510B4 (de) 2004-10-15 2012-01-12 Siemens Ag Verfahren zur Ventilsteuerung bei der Thermozyklisierung einer Substanz zwecks PCR und zugehörige Anordnung
CN107715930B (zh) * 2017-09-22 2020-03-17 华中科技大学同济医学院附属协和医院 芯片结构
JP7668523B2 (ja) * 2021-06-04 2025-04-25 国立研究開発法人産業技術総合研究所 マイクロチャンバ、マイクロチャンバ装置、及びマイクロチャンバの製造方法

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Cited By (13)

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US7431891B2 (en) 2000-11-29 2008-10-07 Merck Patent Gmbh Device for controlling the temperature of chemical microreactors
US20040028562A1 (en) * 2000-11-29 2004-02-12 Thomas Greve Device for controlling the temperature of microcomponents
US20080047836A1 (en) * 2002-12-05 2008-02-28 David Strand Configurable Microfluidic Substrate Assembly
US20050006372A1 (en) * 2003-07-10 2005-01-13 Citizen Watch Co., Ltd Temperature regulator for microchemical chip
US7244913B2 (en) 2003-07-10 2007-07-17 Citizen Holdings Co., Ltd. Temperature regulator for microchemical chip
US7691334B2 (en) 2005-09-20 2010-04-06 Yamaha Corporation Temperature control apparatus for microchemical chip
US20070116614A1 (en) * 2005-09-20 2007-05-24 Yamaha Corporation Temperature control apparatus for microchemical chip
US20130015254A1 (en) * 2011-07-13 2013-01-17 GM Global Technology Operations LLC Temperature dependent variable flow orifice
US9618132B2 (en) * 2011-07-13 2017-04-11 GM Global Technology Operations LLC Temperature dependent variable flow orifice
US20140227147A1 (en) * 2013-02-08 2014-08-14 Infineon Technologies Ag Microfluidic Device and Method
US10086370B2 (en) * 2013-02-08 2018-10-02 Infineon Technologies Ag Microfluidic device and method
USD844805S1 (en) 2016-02-29 2019-04-02 President And Fellows Of Harvard College Holder
USD846755S1 (en) * 2016-12-07 2019-04-23 President And Fellows Of Harvard College Holder

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WO2000048724A1 (fr) 2000-08-24
EP1174182A1 (fr) 2002-01-23
KR20020003368A (ko) 2002-01-12
AU2571600A (en) 2000-09-04
KR100630297B1 (ko) 2006-09-29
CN1341041A (zh) 2002-03-20
EP1174182A4 (fr) 2003-07-23
CA2371767C (fr) 2007-05-08
CA2371767A1 (fr) 2000-08-24
CN1150059C (zh) 2004-05-19

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